Reacción #71865

ord-47c782a9394549e481b52eb2e7a2fe4e

Disolventes

Condiciones de reacción

Temperatura
100°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    FiltraciónThe insoluble matter was filtered off
  2. 2
    workup.ADDITIONethyl acetate was added to the mother liquor
  3. 3
    Lavadothe organic layer was washed with water and brine
  4. 4
    Secadodried over anhydrous magnesium sulfate
  5. 5
    ConcentraciónConcentration under reduced pressure

Procedimiento

DMF (5 mL), water (5 mL), zinc (0.7 g, 10.7 mmol) and iron trichloride hexahydrate (0.12 g, 0.4 mmol) were added to methyl 3-[(7-nitro-2,3-dihydro-4H-1,4-benzoxazin-4-yl)methyl]benzoate obtained in Example (100a) (0.35 g, 1.07 mmol), and the mixture was stirred at 100° C. for 50 minutes. The insoluble matter was filtered off and ethyl acetate was added to the mother liquor, and the organic layer was washed with water and brine, and dried over anhydrous magnesium sulfate. Concentration under reduced pressure gave 0.28 g of the crude title compound as a brown oily substance (88%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08536197B2uspto-grants-2013_09